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Vol. 58and concentrated. There resulted a viscous yellow oil boiling at 280-285°( 2 mm.). The yield was 4.4 g. or 84.1%. Anal. Caled, for CuHieOaBr: C, .5; , 4.1; -OCHs, 9.8. Found; C, 60.8; , 4.0; -OCHs, 10.0.o-Bromophenylglyoxylic Acid.-This acid was purified by several crystallizations from methyl alcohol and water. The thin colorless needles melted over a range with decomposition as reported by Russanow. For a concentra-tion of 0.03449, molecular conductivity 266.21, and conductivity at infinite dilution 348, the ionization constant at 25°was calculated to be 8.6 X 1Q-Z.

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Recently there was reported2 a general method for the production of alkyl peroxides and hydroperoxides. However, no extensive study has been made of this method, nor have any attempts been made to isolate other peroxides than alkyl hydroperoxides. The present investigation reports a careful study of this reaction, the isolation of two of the peroxides formed and a study of some of their properties.The process simply involves the reaction, in the cold, of an alkyl hydrogen sulfate with a concentrated solution of hydrogen peroxide. For example, when molar quantities of ¿-butyl alcohol or isobutylene are allowed to react, in the cold, with sulfuric acid (70%) and an equivalent quantity of 30% hydrogen peroxide is slowly added, a mixture is obtained which contains 50-70% tbutyl hydroperoxide. A careful fractionation of this mixture under reduced pressure yields, in addition to ¿-butyl hydroperoxide, an appreciable amount (30-50%) of di-¿-butyl peroxide boiling at 12-13°( 20 mm.), or 109-109.2°( 760 mm.).From the same mixture one can also separate this peroxide in relatively pure form by extracting the hydroperoxide, either with a strong alkali solution or several times with water. By adjusting the concentration of sulfuric acid one can obtain this peroxide in 85% yield. Furthermore, it can be prepared in 92% yield by allowing ¿butyl hydroperoxide to react with ¿-butyl hydrogen sulfate.

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